CN107413294A - A kind of method that graphene-supported silver handles high Oil repellent domestic water - Google Patents
A kind of method that graphene-supported silver handles high Oil repellent domestic water Download PDFInfo
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- CN107413294A CN107413294A CN201710358474.7A CN201710358474A CN107413294A CN 107413294 A CN107413294 A CN 107413294A CN 201710358474 A CN201710358474 A CN 201710358474A CN 107413294 A CN107413294 A CN 107413294A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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- Carbon And Carbon Compounds (AREA)
- Water Treatment By Sorption (AREA)
Abstract
A kind of graphene-supported silver handles high Oil repellent domestic water method, the 30ml of graphene oxide 20 that (1) takes, the 5ml of silver nitrate 3 is added dropwise, ultrasonic mixing is made in stirring, NaOH solution thing cooling to be mixed is added dropwise, filtering, washing, alcohol are washed, and AgNO is then added dropwise3Side is stirred, and ammoniacal liquor is added dropwise into solution without precipitation in side, and formaldehyde, insulation reaction 2 hours is added dropwise;(2) step (1) product is poured into centrifuge tube, 5min, standing separation is centrifuged under 8000 turns, washing, alcohol are washed each 3 times, 80 DEG C of holding drying 3 hours in an oven;The present invention prepares graphene-supported silver using cheap carbon material.It is nontoxic to human body, environmentally safe to prepare material;Process conditions are simple, safety, energy-conservation.
Description
Technical field
The present invention relates to water treatment field, more particularly to a kind of graphene-supported silver handles high Oil repellent domestic water side
Method.
Background technology
Water is Source of life.With population be continuously increased and industrial expansion, the mankind to the utilization scope of water resource not
Disconnected to expand, water consumption increases year by year, and water resources crisis signals for help repeatedly.Fluorine is the necessary trace element of human body, participates in system in vivo
The physiological activity of row, it is the part of tooth and bone, it is required for body normal calcification, normal reproductive function, to human body
For, its concentration in human body depends on external environment situation, when fluorinated volume is high in environment, fluorinated volume in particularly drinking water
The intake of human body is just more when high, when environment lacks fluorine, also lacks therewith in vivo.Adult, daily can be from general under positive reason
The fluorine needed for physiology is obtained in logical drinking-water, diet, because the fluorine obtained in drinking-water is almost absorbed completely.Therefore in drinking water
Influence of the content to health has conclusive effect.But high-fluorine water ought be drunk for a long time, gently can then cause fluorosis of bone and fluorine
Dental plaque, heavy then can cause osteosclerosis or osteoporosis, textured bone, or even paralysis, make one disability.Therefore this is worked as
When Oil repellent is too high in a little drinking-water, the comprehensive preventive health measures such as reducing fluoride content and improving water quality must be taken again.Sewage disposal is carried out, realizes that sewage provides
Source, the utilization rate of water resource can be increased substantially.
Recent domestic is to fluorinated water mainly using three kinds of chemical precipitation, flocculation sediment, absorption handling process.Chemistry is heavy
Shallow lake method typically uses calcium salt precipitation method, i.e., the feeding lime into waste water, fluorine ion is generated CaF with calcium ion2Precipitate and remove
Go.The technique has the advantages such as method is simple, processing is convenient, expense is low, but it is difficult up to standard, body refuse sedimentation to deposit water outlet after treatment
The shortcomings of slowly and dehydration is difficult.The conventional flocculant of the flocculent precipitation of fluorine ion waste water is aluminium salt.Aluminium salt is added in water
Afterwards, Al is utilized3+Complexing and aluminium salt hydrolysis intermediate product and the Al (OH) ultimately produced with F-3.Compared with calcium salt precipitation method,
Aluminium salt flocculent precipitation have added amount of chemical is few, treating capacity is big, after single treatment up to discharging standards the advantages of.Aluminium salt
Flocculent precipitation there is also it is obvious the shortcomings that, i.e., use range is small, if fluorinated volume is big, coagulant usage amount is more, processing cost
It is larger, it is more to produce sludge quantity;F- removal effects SO in by the operation factors such as stirring condition, sedimentation time and water4 2-, Cl-Deng it is cloudy from
Son is had a great influence, and effluent quality is not sufficiently stable, but dosage is big, it need to add 150 per cubic meter of water according to different situations~
1000g, this can make to contain a certain amount of dissolving aluminium to human health in water outlet.
Absorption method is to handle the effective ways of low concentration fluoride waste.Adsorption method because of easy to operate, high treating effect and
The advantages such as expense is low are widely used in environmental pollution improvement, and from long-range angle analysis, this is that to solve global water resources short
Lack the standard for reaching drinking water with the effective way of water environment degradation.The active aluminum oxide of conventional adsorbent, clinoptilolite, work
Property charcoal etc..But the adsorption capacity of these sorbing materials is not high, and regenerate difficult.
The content of the invention
In order to overcome above-mentioned technical weak point, the invention provides a kind of graphene-supported silver to handle high Oil repellent
Domestic water method, the composite using graphene as substrate, based on the huge specific surface area of graphene, impart graphene more
Add excellent performance, graphene-supported silver both adds adsorption effect as adsorbent, adds antibiotic property again, it is used for high fluorine
Content domestic water, has broad application prospects.
In order to achieve the above object, the technical proposal of the invention is realized in this way:
A kind of graphene-supported silver handles high Oil repellent domestic water method, comprises the following steps:
(1) 2mmol/L-6mmol/L graphene oxide 20-30ml is taken, 10mmol/L silver nitrate 3-5ml, ultrasound is added dropwise
30min is mixed, under magnetic agitation effect, 4mol/L NaOH solution 7ml-10ml are added dropwise, react 15min, thing to be mixed is cold
But, filter, wash, alcohol is washed each 3 times, subsequent dropwise addition 0.05M AgNO33-5ml sides are stirred, and 2% ammoniacal liquor is added dropwise into solution in side
Without precipitation, the formaldehyde 1ml of mass fraction 37%, insulation reaction 2 hours is added dropwise;
(2) step (1) product is poured into centrifuge tube, 5min, standing separation is centrifuged under 8000 turns, washing, alcohol wash each 3
Time, 80 DEG C of holding drying 3 hours in an oven.
Positive benefit:
(1) graphene-supported silver is prepared using cheap carbon material.Prepare material it is nontoxic to human body, to environment without dirt
Dye.
(2) high Oil repellent domestic water is handled using graphene-supported silver, process conditions are simple, safety, energy-conservation.
(3) the graphene-supported silver prepared is to low with antibiotic property, cost.
(4) the method is used to handle high Oil repellent domestic water, and the clearance of fluorine can greatly reduce height up to more than 90%
Fluorinated volume in Oil repellent domestic water, it can solve the problem that the puzzlement that high fluorine-containing domestic water is brought to local people's domestic water.
Brief description of the drawings
Fig. 1 is the standard curve that the ion selective electrode method of embodiment one determines fluorine ion.
Embodiment
The invention will now be described in detail with reference to the accompanying drawings.
Embodiment one
The present embodiment comprises the following steps:
(1) 5mmol/L graphene oxide 25ml is taken, 10mmol/L silver nitrate 4ml, ultrasonic mixing 30min, in magnetic is added dropwise
Under power stirring action, 4mol/L NaOH solution 7ml are added dropwise, react 15min, thing cooling to be mixed, filtering, washing, alcohol wash each 3
Time, 0.05MAgNO is then added dropwise34ml sides are stirred, and 2% ammoniacal liquor is added dropwise into solution without precipitation in side, and the first of mass fraction 37% is added dropwise
Aldehyde 1ml, insulation reaction 2 hours;
(2) step (1) product is poured into centrifuge tube, 5min, standing separation is centrifuged under 8000 turns, washing, alcohol wash each 3
Time, 80 DEG C of holding drying 3 hours in an oven.
Graphene-supported silver-colored 150mg manufactured in the present embodiment is dissolved in 1L fluorinated waters, ultrasonic vibration 30min, in level
Shaker at room temperature shakes 5 hours, stands, filtering.Content of fluoride ion in water is determined with ion selective electrode method.Method for measuring
It is as follows:
A, fluorine standard reserving solution (5.26*10 is prepared-5mol/L):NaF0.2210g accurately is weighed, is dissolved in deionized water,
Move into 1000mL volumetric flasks, be diluted to scale with deionized water, shake up.
B, total ionic strength cushioning liquid (TISAB) is prepared:500mL deionized waters are added in 1000mL beakers, then are added
Enter 50mL glacial acetic acid, 12g sodium citrates, 58gNaCl stirrings are allowed to dissolve, beaker is placed in cold bath, will with ammoniacal liquor (1+1)
Solution is adjusted to Ph5.0-5.5, compares pH test paper, is finally diluted to 1L. with deionized water
C, fluorine standard liquid (5.26*10 is prepared-4mol/L):By fluorine standard reserving solution (5.26*10-5Mol/L) spend from
Sub- water dilutes 10 times.
D, preparing standard solution:Fluorine standard liquid (5.26*10 is weighed respectively-4Mol/L) 0.90ml, 1.40ml,
It is molten to add TISAB in 9 50mL volumetric flasks by 1.90ml, 2.40ml, 2.90ml, 3.30ml, 3.80ml, 4.30ml, 4.80ml
Liquid 10mL, is diluted to scale with deionized water, shakes up, that is, it is respectively 1*10 to obtain concentration-5Mol/L, 1.5*10-5Mol/L, 2*
10-5Mol/L, 2.5*10-5Mol/L, 3*10-5Mol/L, 3.5*10-5Mol/L, 4*10-5Mol/L, 4.5*10-5Mol/L, 5*10- 5Mol/L standard serial solution.
E, standard curve is drawn, as described in Figure 1:The solution of least concentration in standard serial solution is transferred to dry plastics bottle
In, into indicator electrode and reference electrode, one-shot battery electromotive force (E) is read every half a minute, until reading is basic in 1min
(< 1mV).Tested one by one from low concentration to high concentration, and draw standard curve, calculate regression equation.
According to Fig. 1 fluorine ion standard curve, Oil repellent 10 is taken-5Exemplified by M, adsorption rate adsorption rate=(C is calculated1-C0)/
C1, such as following table.
Embodiment two
The present embodiment comprises the following steps:
(1) 4mmol/L graphene oxide 25ml is taken, 10mmol/L silver nitrate 3ml, ultrasonic mixing 30min, in magnetic is added dropwise
Under power stirring action, 4mol/L NaOH solution 7ml are added dropwise, react 15min, thing cooling to be mixed, filtering, washing, alcohol wash each 3
Time, 0.05M AgNO are then added dropwise33ml sides are stirred, and 2% ammoniacal liquor is added dropwise into solution without precipitation in side, and mass fraction 37% is added dropwise
Formaldehyde 1ml, insulation reaction 2 hours;
(2) step (1) product is poured into centrifuge tube, 5min, standing separation is centrifuged under 8000 turns, washing, alcohol wash each 3
Time, 80 DEG C of holding drying 3 hours in an oven.
Graphene-supported silver-colored 150mg manufactured in the present embodiment is dissolved in certain 1L fluorinated waters, ultrasonic vibration 30min,
Room temperature is shaken 3 hours on horizontal oscillator tube, is stood, filtering.Content of fluoride ion in water, experiment card are determined with ion selective electrode method
Bright graphene-supported silver is used to adsorb fluorine ion in water, works well, adsorption rate can make high Oil repellent drinking water up to more than 90%
Reach drinking water standard.Graphene-supported silver is safe and non-toxic, and the bactericidal action of silver, it is more showed potential application value
Embodiment three
The present embodiment comprises the following steps:
(1) 2mmol/L graphene oxide 20ml is taken, 10mmol/L silver nitrate 3ml, ultrasonic mixing 30min, in magnetic is added dropwise
Under power stirring action, 4mol/L NaOH solution 7ml are added dropwise, react 15min, thing cooling to be mixed, filtering, washing, alcohol wash each 3
Time, 0.05MAgNO is then added dropwise33ml sides are stirred, and 2% ammoniacal liquor is added dropwise into solution without precipitation in side, and mass fraction 37% is added dropwise
Formaldehyde 1ml, insulation reaction 2 hours;
(2) step (1) product is poured into centrifuge tube, 5min, standing separation is centrifuged under 8000 turns, washing, alcohol wash each 3
Time, 80 DEG C of holding drying 3 hours in an oven.
Graphene-supported silver-colored 100mg manufactured in the present embodiment is dissolved in certain 1L fluorinated waters, ultrasonic vibration 30min,
Room temperature is shaken 3 hours on horizontal oscillator tube, is stood, filtering.Content of fluoride ion in water, experiment card are determined with ion selective electrode method
Bright graphene-supported silver is used to adsorb fluorine ion in water, works well, adsorption rate can make high Oil repellent drinking water up to more than 90%
Reach drinking water standard.Graphene-supported silver is safe and non-toxic, and the bactericidal action of silver, it is more showed potential application value
Example IV
The present embodiment comprises the following steps:
A kind of graphene-supported silver handles high Oil repellent domestic water method, comprises the following steps:
(1) 6mmol/L graphene oxide 30ml is taken, 10mmol/L silver nitrate 4ml, ultrasonic mixing 30min, in magnetic is added dropwise
Under power stirring action, 4mol/L NaOH solution 8ml are added dropwise, react 15min, thing cooling to be mixed, filtering, washing, alcohol wash each 3
Time, 0.05MAgNO is then added dropwise35ml sides are stirred, and 2% ammoniacal liquor is added dropwise into solution without precipitation in side, and mass fraction 37% is added dropwise
Formaldehyde 1ml, insulation reaction 2 hours;
(2) step (1) product is poured into centrifuge tube, 5min, standing separation is centrifuged under 8000 turns, washing, alcohol wash each 3
Time, 80 DEG C of holding drying 3 hours in an oven.
Graphene-supported silver-colored 180mg manufactured in the present embodiment is dissolved in 1L fluorinated waters, ultrasonic vibration 30min, in level
Shaker at room temperature shakes 10 hours, stands, filtering.Content of fluoride ion in water is determined with ion selective electrode method.Experiment proves
Graphene-supported silver is used to adsorb fluorine ion in water, works well, adsorption rate can reach high Oil repellent drinking water up to more than 90%
To drinking water standard.Graphene-supported silver is safe and non-toxic, and the bactericidal action of silver, it is more showed potential application value
Embodiment five
The present embodiment comprises the following steps:
(1) 6mmol/L graphene oxide 30ml is taken, 10mmol/L silver nitrate 5ml, ultrasonic mixing 30min, in magnetic is added dropwise
Under power stirring action, 4mol/L NaOH solution 10ml are added dropwise, react 15min, thing cooling to be mixed, filtering, washing, alcohol are washed respectively
3 times, 0.05MAgNO is then added dropwise35ml sides are stirred, and 2% ammoniacal liquor is added dropwise into solution without precipitation in side, and mass fraction 37% is added dropwise
Formaldehyde 1ml, insulation reaction 2 hours;
(2) step (1) product is poured into centrifuge tube, 5min, standing separation is centrifuged under 8000 turns, washing, alcohol wash each 3
Time, 80 DEG C of holding drying 3 hours in an oven.
Graphene-supported silver-colored 200mg manufactured in the present embodiment is dissolved in 1L fluorinated waters, ultrasonic vibration 30min, is shaken in level
Swing room temperature on device to shake 12 hours, stand, filtering.Content of fluoride ion in water is determined with ion selective electrode method.Experiment proves stone
Black alkene load silver is used to adsorb fluorine ion in water, works well, adsorption rate can reach high Oil repellent drinking water up to more than 90%
Drinking water standard.Graphene-supported silver is safe and non-toxic, and the bactericidal action of silver, it is more showed potential application value.
Claims (2)
1. a kind of graphene-supported silver handles high Oil repellent domestic water method, it is characterised in that comprises the following steps:
(1) 2mmol/L-6mmol/L graphene oxide 20-30ml is taken, 10mmol/L silver nitrate 3-5ml, ultrasonic mixing is added dropwise
30min, under magnetic agitation effect, 4mol/L NaOH solution 7ml-10ml are added dropwise, react 15min, thing cooling to be mixed, mistake
Filter, washing, alcohol are washed each 3 times, and 0.05M AgNO are then added dropwise33-5ml sides are stirred, and 2% ammoniacal liquor is added dropwise into solution without heavy in side
Form sediment, the formaldehyde 1ml of mass fraction 37%, insulation reaction 2 hours is added dropwise;
(2) step (1) product being poured into centrifuge tube, 5min, standing separation is centrifuged under 8000 turns, washing, alcohol are washed each 3 times,
80 DEG C of holding drying 3 hours in an oven.
2. the graphene-supported silver of one kind according to claim 1 handles high Oil repellent domestic water method, it is characterised in that
Comprise the following steps:
(1) 5mmol/L graphene oxide 25ml is taken, 10mmol/L silver nitrate 4ml are added dropwise, ultrasonic mixing 30min, are stirred in magnetic force
To mix under effect, 4mol/L NaOH solution 7ml are added dropwise, react 15min, thing cooling to be mixed, filtering, washing, alcohol are washed each 3 times, with
After 0.05MAgNO is added dropwise34ml sides are stirred, and 2% ammoniacal liquor is added dropwise into solution without precipitation in side, and the formaldehyde of mass fraction 37% is added dropwise
1ml, insulation reaction 2 hours;
(2) step (1) product being poured into centrifuge tube, 5min, standing separation is centrifuged under 8000 turns, washing, alcohol are washed each 3 times,
80 DEG C of holding drying 3 hours in an oven.
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Cited By (1)
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CN111841496A (en) * | 2020-07-24 | 2020-10-30 | 泉州南京大学环保产业研究院 | Method for rapidly preparing silver-loaded activated carbon |
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